Appabattts fob testing complex liquids



A. T. SAUNDERS.

APPARATUS FOR TESTING COMPLEX LIQUIDS.

APPLICATION FILED JULYIH. 1916.

1,307, 60 1 Patented June 24, 1919.

2 SHEETS-SHEET I.

as 1 2s Fig.2.

W I TNESSES: IN VEN TOR.

A. T. SAUNDERS.

APPARATUS FOR TESTING COMPLEX LIQUIDS. APPLICATION FILED 1uL'Y3l,1916.

1,307,60 l Patented June 24; 1919.

2 SHEETS-SHEET 2 1 w ms B N E- snmson rjsannnnns, or oHIcoPEE; msssncrosm'rs.

To all whom. it may concern:-

"nuance-r03. manna comrtnx mourns.

Be it known that .I, AomsonT smunm a citizen of the United States, and a resident of Chicopee, in the county and State of Massachusetts, ha 'e' imgented certain new and useful Impro ements 1n Apparatus for Testing-Complex Liquids, of-

which the following is a specification.

My "invention relates to apparatus for distillin It is designed ,for the distillation upon a laboratory scale of liquids of. a complex nature concerning which itis desired that the relative and actual quantities of the various portions having diflerent boiling points shall be determined together .with the temperatures at which they volatilize.

A prlncipal object of my invention, is to provide means of securing more; uniform and accurate records of results in the fractional distillation of liquids than are obmaybe applied to its under portion.

thermometer is mounted in the neck of thetained by present methods.

, Another object is to cheapen the making of tests of complex liquids by fractional distillation in the laboratory.

A method and apparatus at present com.- monly employed in making fractional. distillations on a laboratory scale areas follows: The fluid to be distilled is placed inaflask so mounted or supported that heat,

A care and accuracy of observation of the flask, enabling the observation of the temperatures at which contents volatilize, and the neck of the flask also has a tube through which such volatilized portions pass over into a condenser.

This condenser consists of a spiral tube, or a some equivalent, surrounded by a vessel through which cold water is caused to flow.

The volatilized liquid passing into the tube,

is condensedby cooling and discharges into a graduated receptacle. When a distillation is to be made with such an apparatus heat is applied tothe fluid in the flask, raising its temperature 'until the first of the distillatethat portion of theliquid having the lowest boiling pointbegins to come.

over, or' appear in the receiver. The temperature 1s noted and maintained until -no more distillate passes over. The amount which has distilled is also recorded. The temperature'is then raised through a certain interval or until the fractlon which 'is volat1lizable at this second joint begins to come over, and, is again maintained w1th-.

oi Hampden various portions of the- I Patented J une '24=, 1919. Application and m 31, 19.16. smhiminaau.

out further increase until nomore fluid distils. Again thetemperature andthe quantity of the fraction are recorded,-and

this procedure is continued until all the various fractions have been distilled-with the exception sometimes-of a er cent. of heavy residue -andtheir quantities and the temperatures at which they volatilizehave been recorded. A modification of is maintained,witli a constantly increasing temperature and without interruption, from the beginning of distillation. The quantity which comes over while the temperature.

a this-procedure is .fre quently employed, as follows: The boiling rises through acertain interval or number of degrees is collected in a receptacle, that fraction which distils while themercury.

- rises through asecondf and equal interval is manipulator. Since the personal equation enters unavoidably into the matter more or less inaccuracy must result, making difficult the fixing or determining of standards, commercial or technical.

My invention provides means for avoiding these inaccuracies; eliminating the personal equation and securin practlcally uniform and exactv results. and autographically charts the curve of the operation as it proceeds; It enables the carrying on of numerous distillations simultaneously by a single operator and without {the constant attention required by present methods.

The manner in which I preferftojcarry out my invention is illustrated in the accompanying drawings, which are somewhat in outline and partly diagrammatic.

Figure 1- is a general view' of an apparatus arranged and constructed in accordance with my invention.

Fig. 2 shows the-laminated coil 43 in plan. Figs. 3 and 4 are illustrative of portions of-charts of the character preferably used t automatically echartsas' my invention, and-or the-curvea-t raced' the well known forms of recording therduringlthe -operat oxi thereof. It. w1 ll be mometers, etc. A similar cylinder, 36, bearunderstood-f.thatfthenumerals on 'the m'ar s iug a similar chart 87 is driven from the ottheseilatter representthose o the shaft of the cylinder 83 at the same speed ,snu are indicative divithrough the pairs of gears 38 and .38'uand 70 sions for egree's'oi rature, periods of the'shaft 39. The en arm 40 is afiixed to tiifi'e and 'uantitiesoft efractions-of'dlsthe shaft 41 which is rotatable 'in asuitable 1 'tillate, are {not to be con-fused with the mounting 42 closing the mouth of the flask reference" numerals ofthe'drawinge. They 1 in which it is firml seated. To the lower .1 will, howeyen'; lie-separately referred to in end of the shaft 41 1s aflixed the inner ex- 16' 'th1s'-*des'criptio I g c tremity of the laminated coil 43, its outer It is not nry to illustrate all the extremity being aflixed to the mounting 42 forms in which the invention may be carried by the pm- 44. This laminated coil 43, the outandI have' therefore shown only the narm andthe rotating cylinder" 86 16 preferred ap aratus for the laboratory. r earmg a chart are all similar to correspond In .Fig.' -1. e body of the still is a glassmg parts 111 a well known form of recording 4 flaskl'l mounted upon th'e'support 2. 8 is a thermometer, which they in fact constitute oondenser'of glass comprising a spiral tube in time device. v or .worm 'aud an inc osing vessel having In practice the laminated coil 48 is mount- 20 the inlet 4." and the outlet 4, the former beed somewhat lower in the throatof the flask ing-oonnected witha suitable sourceof cold than shown, to bring 1t into the current of water "supplyl and the, latter t wa te, vapor passing over into the outlet of the, v e

through flexi tubing,.broken away in the flask. I i

drawings The condenser is mounted upon Forclearness of illustration and to avoid 25 the support 6, its spiral tubebeing connected crowding 1n the drawm the cylinder 38 at its upperextremity in the usual way with carrying the chart 35 1s s own in a position the tube leading from the head of the still relative to the float 28 making the connection at 6 and discharging at 7. Upon the support of the rod 32 to be with the pen arm proper.

6 is pivoted at 8 the arm 9'having clamps 10, It lS 0bV10l1S that the principle is the same 80 10' in which the tube 11 is held. This tube as if the rod'were connected to the short arm has aiunnel-shaped mouth 12 and at its at an equal distance from the fulcrum 31. other end a bulbous enlargement 13'having In the position the resultant movement of an opening 14 in its top and a dischargigg the pen would be downward as the float aperture 15. a The arm 9 is counterbalan rises, and this is the arrangement of parts 35 by the adjustable weight 16 and the .coil preferred in practice, the balancing weight spring 17 this spring ingattached to the 29 being adjusted on the pen arm proper, 30. arm- 9 through its clam 10 and at its upper It is 1n consonance with this latter arrangeend to the screw 18 which travorseslaninsument of parts that the accompanying draw-' lated bearing in the arm 19 and carries the lugs of portions of charts, Figs. and 4 are i 40 knurled nut 20. Thearm'19 is aflixed to the made. I The movement of hfufwn a m 40 support 5 but, insulated therefrom. Its being in the direction indie by. the ardowncurved point. 21 and the upcurved point row, Fig. 2, and of the cylinders as similarly 22 of the arm 9 form contacts in the circuit indicated in Fig. 1. It will be understood 23, 23, etc. The current for this circuit is that it is immaterial whether this latter ar- 45 supplied from any suitable sources-dynamo rangement be used with the chart 35 or the 11-0 *or battery-indicated at 24. The arm 9 is cylinder 33 be located'to the left of the float insulated from the support 5 at the pivotal rod and of the fulcrum 31'. If this chan point 8, the connection ofthis arm with the in relative positions of these members e circuit 28 being through its. bearing at this made, the connection of the float rod with to point. In the circuit 23 isalso the laminated. the pen arm would then be at the point 116 the'rmo-electric cutout 25 mounted on the shown in the drawing, in order that the flask'l. A voltage regulator, indicated at X, movement of the gen should be from the may be introduced into the circuit, which lower toward the igher numbered spaces.

also supplies the thermo electric element-.- on the chart.

i "55 electric heater-26} The operationof the apparatus is as fol- 27 is a receptacle for distillate and is' lows shown, as is also the flask 1, as containin The liquid to be distilled is placed in the liquid. 28 is a float borne up by the disti flask 1, a certain carefully measured quanlate andby the balancing weight 29 adjusted tity being used. The weight 16 and the 60 to that function on the shorter arm or lever spring 17 are so adjusted as to hold .the

of the pen arm 30 which is pivoted at 31 and contact points 21 and 22 lightly together connected with the float 28 by the rod 32. when there is no liquid in the tube 11. Cold 33 is a cylinder rotated by the clock mechawater is turned into the condenser 3 through nism 34 and adapted to carry the chart 35, the inlet-4' in continuous flow, exhausting 06 similar to the chart and cylinder elements of through 4. The float 28 rests at the bottom of the receptacle 27, balanced by the weight 29. The chart 35 is placed on the cylinder 33 and the chart 37 upon the cylinder 36, the inked pens of-3O and 40 restin upon charts at proper starting points, in icated by mp and new in Figs. 3 and 4 respectively. The current from 24 is turned on through the circuit 23, steadily raising the temperature of the heater 26 and with it that of the liquid in the flask 1. As this begins to -volatilize, the heated vapor acts upon the coil 43 causing the pen of arm'40 to begin to trace the line upon the chart 37 indicating and recording such rise. Simultaneously with the beginning of volatilization the clock -mechanism 34 is started, rotating .the cylinders 33 and 36. I may, when desirable, employ an automatic starter, electric, forthe clock, actuated by the first flow of distillate in the tube. but do not wish to. complicate these specifications with this in detail. As the liquid 'volatilizes, the vapor passes over into the condenser 3'reliquefying and discharging from the worm at 7 into the funnel shaped mouth 12 of the tube 11 and flowing into the bulbous end 13, thence through the orifice 15 into the receptacle 27. The size of the aperture 15 is such that with a rate of flow of distillate calculated to result there will be no accumulation in the bulb in complete distillation of the contents of the flask 1 in the period of a single revolution of the record cylinders 33 and 36,

i '13, but such that when this flow increases beyond the desired rate such accumulation occurs. The adjustment above described beingsuch that the contact points 21 and 22 are'but lightly held together when this bulb is empty, the accumulation in the latter promptly parts them by depressing the tube '11, and thus opens the heating circuit 23, thereby retarding the rise of temperaturein the flask. 'In order that the results shall be immediate uponthe temperature of the liquid in the flask, or, more accurately, upon thefrate of volatilization, the heater 26 is, constructed without superfluous metal,,and

- with the electric coil in as direct and comrent occasioned b .plete contact as practicable withithe bottom of the flask. Any excess in the accu-- mulation of distillate beyond the capaci-' ties of the bulb overflows through the opening 14 in the top of the same and discharges with the rest into the receptacle 27 It will be understood that except for, andduring, the interruptions of the heating curthe action of excessive How of distillate 1n opening the circuit 23, as described, the temperature in flask 1 con stantly increases from the beginning of the operation to its completion. In making fractional distillations of samples 9f such .complex fluids as'petroleum products, a

limit is usually predetermined beyond which the heat will not be carried; observation sents fractions of distillate.

bring the record of an entire. operation with being made of the per cent. of residue which will not come over at this point.

vIn my invention, the thermo-cutout25 is set for this predetermined point and, in the event of failure ofthe operator to cut off 'the current when this temperature is reached, the cutout prevents a furtherrise by opening the circuit 23. This maintains the temperature at this point. One of the Well known forms of circuit breakers may the charts 35 and 37 are similarly divided into spaces representing in both certain periods of time and also in the case of chart 35 certain quantities and in-that of 37 certain degrees of temperature, the curves drawn upon these' two charts during an operation constitute a record, to be read conjointly, of

the boiling points of the various fractions of the liquid.

In the illustrations of portions of charts, Figs. 3 and 4, curves have been drawn illustrative of curves for a. hypothetical liquid.

-A's indicated, Fig. 4 represents chart 35 and the curve is that recorded by the pen arm controlled by the float 27, while Fig. 3 represents the chart 37 with the curve recorded by the pen arm controlled by the thermo-coil 43. To make clearer the illustration, the curve of chart 35 is also indicated in dotted line upon chart 37. The charts are divided up in a usual way by lines 'in'two directions, the curved lines having the same. radii as described bythe pens when the cylinders are not moving, and the straight lines whichcross them having the direction of line which the pens trace when they are stationary and the cylinders rotating. The lines of numerals, along the topimargins of the two charts indicate intervals of time divided into periods of five minutes each, thesingle lines representing each one minute. The speed of the clock mechanism is regulated to bring the curved lines under thepens in consonance withthese periods.

The vertical row of numerals on chart 37 indicates degrees. of temperature, each' line representing one degree of change from the next. The vertical row on chart 35 repre- In order to in the range .of the usual pen and cylinder,

these are preferably divided as here, so that each space between lines represents two per cent. of the total liquid. The adjustment of float, rod and pen arm are madein consonance with this.

An examination-of the illustrative charts shows that at the beginning of the o eration the pen of the thermometer reste at mp (Chart 37 and the floatcontrolled pen rested at weep (Chart 35). That is, the thermometer pen at 60, time 0, and the distillate pen at a corresponding point as to time and showing no liquid distilled. The thermo= line runs with the 0 time lineto 69 degrees, showing that the mechanism actuating the cylinders had not been started While the contents of the flask warmed up to this point. The thermo-line now curves toward the next time line, showin that, with the tempera ture still rising t e cylinders have been set in motion .As the line for the distillate does not follow. the 0 per cent. line, as would be the case ifno liquid were distilling, but instead runs obliquely toward the lines indicating the first per cent. of distillation and the first minute of time, it is seen that the actuating mechanism for the c linders was set in motion the instant of the eginning of distillation, and that this was at 69 de rees. In the next five minutes, as may be rea the temperature has risen ten de ees to 79, whi e 8 per cent. of the li aid as istilled. In the five minutes next fo lowing, the term perature rises but five degrees, w ile twelve per cent. of liquid comes over, showing how the increased rate of flow reduces the rate of rise in temperature.

When the float 28, the single receptacle 27 and their coiirdinate (pen arm are used, the latter may be so mo ified and adjusted as to record ugon the same chart with the pen arm 40, di erent inks bein used to make distinguishable the curve 0 one from that of the other.

Instead of the modification suggested above whereby the two pen arms record upon the same chart, two 0 arts may be used in conjunction with a single cylinder, the latter being made of double len hin order to carry both charts. One 0 the charts inay be upon transparent paper. adapted to be overlaid or superimposed upon the other, to enable their being jointly read more conveniently. In the drawings, the fioat rod 32 is shown as apparently without provision for the deviation from the vertical required by the sweep of the pen arm to which it is attached. This is because this red is flexible, as is permitted by its being relieved from endwise pressure, or'thrust. by the balancing weight 29. This rod may, however, be ointed at a point above its guides. In practice the vapors of distillate have not been ignited by the proximity ofthe contacts 21, 22; but

a light air'current or other expedient may be employed as a precaution.

In brief, many modificationsof theapparatus as shown may be made within the pur view of my invention.

The statement herein as to the curves on the charts, in the drawings, representing those of the pen arms controlled by the float and the thermo-coil, should be qualified as to the upper portions of those curves, 'as these are drawn to illustrate the action as it would be with the current applied to the heating .element 26 Without-the interrupting action mometer comprising a marker member (40) and a chart bearing member (36), said marker member bein adapted to be controlled by the volati lzed contents of said still, a condenser, a receptacle for the condensed distillate, a recording element 20mprisrng a marker member (30) and a chart earmg member (33), said marker member 30) being adapted to be controlled by the ow of distillate, and a motor element operatively connected with said chart bearing members (33 and 36) whereby said two chart bearing members may be driven'at redetermined speeds, all substantially as escribed. 2. In an apparatus of the class described the combinatlon of a still, a recording thermometer comprising a marker member (40) and a chart bearing member (36), said marker member bein adapted to be contrplled by the volati ized contents of said Stlll, a condenser, a receptacle for the condensed distillate, a re'cording element comprising a marker member (30) and a chart bearing member (33), said marker member (30) being adapted to be controlled by the flow of distillate, a motor element operatively connected with said chart bearing members (33 and 36) whereby said two chart bearing members may be driven at predetermined speeds, a thermo electric element adapted to heat said still, an electric circuit for said thermo-electric element, and a makeand-break element in said circuit controlled by the flow of distillate, all substantially as described.

3. In 'an apparatus of the class described the combination of a still, a recording therbearing member (33), said marker member (30) being adapted to be controlled by the flow of distillate, a motor element opera tively connected with, said chart bearing members (33 and 36) whereby said two chart bearing members may be driven at predetermined speeds, a thermo electric element adapted'to heat said still, an electric circuit for said thermo-electric element, a makeand-break element in said circuit controlled by the flow of distillate, and a thermo-electrio cut-out in said circuit in juxtaposition with said still and adapted to be adjusted to break said circuit when a predetermined temperature is reached in said still, all sub- 15 stantially as described.

In testimony whereof I have aflixed my signature, in presence of two witnesses.

ADDISON T. SAUNDERS. Witnesses: Y

ABRAHAM E. SNow, S. RICHARD CARusLn. 

